CN113880475A - Red mud-based magnesium phosphate cement and preparation method thereof - Google Patents
Red mud-based magnesium phosphate cement and preparation method thereof Download PDFInfo
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- CN113880475A CN113880475A CN202111242697.XA CN202111242697A CN113880475A CN 113880475 A CN113880475 A CN 113880475A CN 202111242697 A CN202111242697 A CN 202111242697A CN 113880475 A CN113880475 A CN 113880475A
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- red mud
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B12/00—Cements not provided for in groups C04B7/00 - C04B11/00
- C04B12/02—Phosphate cements
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Abstract
The invention discloses a red mud-based magnesium phosphate cement and a preparation method thereof, wherein the corresponding mineral phase composition is C4The preparation of the AF solid solution, MgO, phosphate and a small amount of retarding components comprises two processes: preparing raw materials and preparing cement, wherein the raw materials of the raw materials comprise 30-50 parts of calcium-magnesium components, 30-45 parts of red mud, 10-20 parts of aluminum raw materials and 0.5-2 parts of boron oxide; the preparation component of the cement is 30-50 parts of C4AF solid solution, 20-40 parts of MgO, 15-25 parts of phosphate and 0-10 parts of retarding component. The invention aims to realize the resource utilization of the red mud, and the red mud is introduced into the magnesium phosphate cement to form the cement containing C4The novel magnesium phosphate cement of AF solid solution reduces the requirement of magnesium oxide on magnesium phosphate cement, and simultaneously C4The introduction of the AF solid solution can improve the cement hydration hardening performance and the water resistance, and has obvious low-carbon significance and technical advantages.
Description
Technical Field
The invention belongs to the field of building materials, and particularly relates to red mud-based magnesium phosphate cement and a preparation method thereof.
Background
The magnesium phosphate cement has a series of advantages of early strength, quick hardening, good fluidity, high bonding strength and the like, and is applied to repair, reinforcement, rush repair and rush construction, severe cold environment, nuclear waste solidification and the like in recent years. Magnesium phosphate cement mainly comprises dead burned magnesium oxide, phosphate and a coagulation substance, and compared with portland cement, the cost of each component is high, which is a main factor for restricting the sustainable development of the magnesium phosphate cement. Especially the preparation of dead-burned magnesia generally requires magnesite to undergo a high temperature process above 1600 ℃, and if the transportation costs caused by the concentrated magnesite production areas are taken into consideration, the high energy consumption of magnesia is the most important factor for the high cost of magnesium phosphate cement. Therefore, how to reduce the preparation cost of magnesium oxide is a potential way for realizing sustainable development of magnesium phosphate cement, and the method is the direction of future efforts in the scientific community and the industrial community.
In view of the currently preferred composition ratios of magnesium phosphate cements, the magnesium oxide is in excess and already far exceeds the magnesium oxide to phosphate ratio required for struvite formation, which means that a large amount of magnesium oxide remains unreacted in the late stages of the hydraulic hardening. It is theoretically possible to reduce the amount of magnesium oxide, and it is advantageous from the results of the present study to use some active aluminum-silicon admixtures or inert materials instead of part of the magnesium oxide. However, the prior art approach does not change the composition of hydration products of magnesium phosphate cement, the magnesium phosphate cement belongs to the category of magnesium cementing materials, the fixation of the hydration products also enables the water resistance of the magnesium phosphate cement to be poor and is in the improvement level all the time, and no feasible measure is provided. If the low-cost preparation of the magnesium oxide and the reduction of the content of the magnesium oxide are associated with the change of the existing hydration product of the magnesium phosphate cement, the improvement of the hydration hardening performance and the water resistance of the magnesium phosphate cement can be further realized, which is beneficial to the sustainable development of the magnesium phosphate cement.
The red mud is a large amount of solid waste discharged in the alumina preparation industry, about 1.0-1.8 tons of red mud is discharged when 1 ton of alumina is produced, and China is used as a large alumina producing country, so that a large amount of red mud is discharged every year. Because of its high iron oxide content and red color, it is called red mud. The main chemical composition of red mud is SiO2、Al2O3、CaO、Fe2O3And the content of each oxide in the red mud is different according to different production modes of the alumina. Some attempts have been made to produce ceramsite from red mud, use the ceramsite as cement raw material, directly use the ceramsite as cement admixture and the like, but the red mud contains high content of alkali, so that the problems exist in the practical application process, and the reclamation of the building materials of the red mud is not widely promoted. With the demand of carbon neutralization/carbon peak reaching, the urgent need of ecological society construction, the efficient utilization of red mud has a long way to go.
The defects of the sustainable development of the magnesium phosphate cement and the red mud resource at present mainly comprise: (1) the content of magnesium oxide in the cement needs to be reduced so as to reduce the preparation cost. (2) The hydration product has single composition, the prior technical performance has little influence on the improvement of the water resistance, and the improvement is mainly a temporary solution and a permanent solution. (3) The resource utilization of the building materials of the red mud has various technical feasibility, but the large amount of disposal and utilization of the red mud is not realized at present. The method is a problem worthy of attention if the red mud resource utilization can be associated with the low-cost preparation of the magnesium phosphate cement.
Disclosure of Invention
The invention aims to provide red mud-based magnesium phosphate cement and a preparation method thereof, wherein red mud is used as a raw material carrier to prepare C-containing cement through high-temperature calcination4AF solid solution-MgO mixture component, then with phosphate and a small amount of retarding component to formulate magnesium phosphate cement. Reduces the content of magnesium oxide, C in the magnesium phosphate cement while absorbing the red mud4The introduction of the AF solid solution enables the magnesium phosphate cement to form a new hydration product in the hydration hardening process, so that the magnesium phosphate cement is endowed with good hydration hardening performance and water resistance while the low-carbon preparation of the magnesium phosphate cement is realized.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect of the invention, a red mud-based C is provided4The raw material precursor for preparing the AF solid solution-MgO comprises the following components in parts by weight: 30-50 parts of calcium-magnesium component, 30-45 parts of red mud, 10-20 parts of aluminum raw material and 0.5-2 parts of boron oxide.
Further, the calcium and magnesium component is calcium carbonate, dolomite or magnesite; the aluminum raw material is Al2O3Low grade alumina or aluminum ash with a content of less than 50%. Magnesium, calcium, iron and aluminum elements provided by calcium-magnesium raw materials, red mud and aluminum raw materials are subjected to a proper high-temperature treatment mode to form C4AF solid solution and MgO, wherein C4The ratio of AF solid solution to MgO can be controlled by the ratio between the raw materials.
Further, in the invention, the red mud containing a large amount of alkali metal potassium andsodium to C4Mineralization of AF solid solutions, significant reduction of C4The formation temperature of AF solid solution further promotes the formation of large amount of calcium sulpho-iron aluminate within the range of 1000-1300 ℃. Visible C4The formation temperature of the AF solid solution is relatively low, and the advantage of low carbon is obvious.
Further, the chemical components of the red mud may differ, and one red mud may satisfy C4The stoichiometric proportion of aluminum and iron required for AF solid solutions may also need to be adjusted stoichiometrically by supplementing certain aluminum constituents.
Further, consider C4The temperature required for AF solid solution formation is relatively low, typically at 1200-1300 deg.C, while the low activity of magnesium oxide required for magnesium phosphate cements generally requires higher temperatures in order to prevent C4Over-burning of AF solid solution and simultaneously considering the aspect of energy conservation in the preparation of C4Introducing certain B in the high-temperature process of AF solid solution and MgO2O3. The boron oxide can realize the preparation of the magnesium oxide at a lower temperature, reduce the activity of the magnesium oxide, crystallize the magnesium oxide into large-size crystal grains and simultaneously ensure that C is also contained4The range of temperatures for AF solid solution formation coincides with the range of temperatures for MgO formation.
Further, boric acid can achieve the above effects in addition to the above boron oxide.
Furthermore, all raw materials in the raw material precursor of the red mud magnesium phosphate cement are divided into powder so as to be fully mixed, and the solid phase reaction is complete in the subsequent clinker preparation process.
Further, the pre-homogenized raw material precursor is placed in a high-temperature furnace at 1200-1300 ℃ for calcination to obtain the C-containing material4AF solid solution-MgO mixture.
Further, the aforementioned C4And grinding the mixture of AF solid solution and MgO, and controlling the particle fineness to be below 75 um.
In a second aspect of the present invention, there is provided a method for preparing a red mud-based magnesium phosphate cement, comprising mixing the above-mentioned raw materials C4Preparing novel phosphoric acid from AF solid solution-MgO mixture and phosphate and coagulation-retarding components in certain proportionMagnesium cement.
Further, the novel magnesium phosphate cement comprises the following mineral phase components in proportion: 30-50 parts of C4AF solid solution, 20-40 parts of MgO, 15-25 parts of phosphate and 0-10 parts of retarding component.
Further, said C4AF solid solutions are not of definite stoichiometry, including C2F、C6AF2、C4AF、C6A2F is at least one of the following, and the average composition of the F is C4AF。
Further, in the synergistic preparation of C4A small amount of B is introduced in the process of AF solid solution-MgO2O3This part B2O3The subsequent hydration process can play a certain role in retarding, so the doping amount of retarding components, such as borax and the like, needs to be properly adjusted according to the constructability requirement of the magnesium phosphate cement.
The magnesium phosphate cement belongs to acid-base reaction, and the pH change range is relatively wide in the hydration hardening process and generally fluctuates within the range of 4.0-11.0. Alkali metals sodium and potassium in red mud are usually dissolved in the C4In the AF solid solution, the sodium and potassium have little influence on the formation of struvite which is a main hydration product in the magnesium phosphate cement, and the hydration hardening performance of the magnesium phosphate cement is improved. Pair C4In the case of AF solid solution, the presence of alkali metal sodium potassium makes C4The probability of occurrence of lattice distortion during the formation of AF solid solution is increased, which is advantageous for hydration activity.
Compared with the prior art, the technical scheme provided by the invention has the following beneficial effects:
(1) the red mud is introduced into the magnesium phosphate cement, so that the content of magnesium oxide in the cement can be reduced; the red mud mainly forms C with calcium-magnesium component and aluminum component4AF mineral phase, other substances in the red mud participate in forming inert minerals which do not influence the hydration of the magnesium phosphate cement. From the above perspective, the introduction of the red mud into the magnesium phosphate cement has an obvious low-carbon significance.
(2) The invention also realizes C4Synergistic preparation of AF solid solution and low activity magnesium oxide. In general, phosphoric acidThe magnesium oxide for the magnesium cement is dead burned magnesium oxide, and the forming temperature of the magnesium oxide can meet the requirement of low activity only when the forming temperature is as high as 1600 ℃; c4The AF solid solution can be formed in large quantity at 1200-1400 ℃. In the invention, a small amount of B is introduced in the preparation process of the raw material2O3So that the activity of the magnesium oxide is obviously reduced at a lower temperature, and the magnesium oxide is crystallized into large-size grains, thereby realizing C while introducing the red mud and a small amount of boron oxide4Synergistic preparation of AF solid solution and low activity magnesium oxide.
(3) Magnesium phosphate cement new mineral phase C prepared from red mud raw material precursor4AF also has positive effect on hydration hardening of magnesium phosphate cement, mainly represented by C4The mechanical property of the AF ore phase magnesium phosphate cement is equivalent to that of the traditional magnesium phosphate cement, and the AF ore phase magnesium phosphate cement has self-hydraulicity C4AF also improves the water resistance of magnesium phosphate cement. The above beneficial effects mainly benefit from C4And (3) carrying out chemical reaction on the AF solid solution and other components of the magnesium phosphate cement to form a novel hydrated substance. The invention takes the red mud as C4AF forms the original object of the carrier and is also the innovation of the present invention.
(4) In the prior art, the red mud contains a large amount of alkali metals, which bring certain harm to the hydration and hardening of portland cement, such as surface blooming of concrete. The hydration reaction mechanism of the magnesium phosphate cement is obviously different from that of the portland cement, so that the adverse effect is not needed to be worried about, and the magnesium phosphate cement has another beneficial effect of introducing the red mud.
Detailed Description
In order to make the present invention more comprehensible, the technical solutions of the present invention are further described below with reference to specific embodiments, but the present invention is not limited thereto.
The sources of the raw materials, which are available commercially, are not specifically mentioned in the examples listed in the present invention. The test methods listed are well known to those skilled in the art and are not listed here unless otherwise noted.
Example 1
A red mud-based magnesium phosphate cement and a preparation method thereof comprise the following steps:
(1) the raw material is prepared by uniformly mixing 45.5 parts by weight of dolomite, 38 parts by weight of red mud, 15 parts by weight of aluminum ash and 1.5 parts by weight of boron oxide, grinding and sieving with a 100-mesh sieve.
(2) Placing the homogenized raw material obtained in the step (1) in a high-temperature furnace for calcining, raising the temperature from room temperature to 1250 ℃ and preserving the temperature for 20min, taking out the calcined material after the program control is finished, and quickly cooling to obtain the material containing C4Mixed mineral phases of AF and MgO.
(3) And (3) grinding the material cooled in the step (2) to control the fineness to be below 75 um.
(4) C to be obtained4And (3) mixing the AF solid solution-MgO mixture with ammonium dihydrogen phosphate and borax according to a ratio of 35:38:20:7 to obtain the final novel magnesium phosphate cement.
Mixing the novel magnesium phosphate cement and water according to the water-cement ratio of 0.19 to form cement paste, adopting a cement mortar mixer, firstly slowly stirring for 1min during mixing, then quickly stirring for 3min, pouring into a cement mortar test mold after stirring is finished, and curing in the air to a specified age. The compressive strengths of tests 1d, 7d and 28d were 39.46 MPa, 65.72 MPa and 75.19 MPa, respectively.
Example 2
A red mud-based magnesium phosphate cement and a preparation method thereof comprise the following steps:
(1) in parts by weight, 25 parts of high-magnesium limestone, 20 parts of magnesite, 37 parts of red mud, 16 parts of aluminum ash and 2 parts of boron oxide are uniformly mixed in advance, ground and sieved by a 100-mesh sieve to obtain a raw material.
(2) Wetting the raw material obtained in the step (1) with proper amount of water, preparing into a cylindrical test cake under certain pressure, drying in an oven, calcining the raw material in a high-temperature furnace, slowly raising the temperature from room temperature to 1300 ℃ and keeping the temperature for 15min, and rapidly cooling the calcined material in the air to obtain C4Mixed ore phase of AF and MgO.
(3) And (3) grinding the material cooled in the step (2) to control the fineness to be below 75 um.
(4) C to be obtained4AFAnd mixing the solid solution-MgO mixture with ammonium dihydrogen phosphate and borax according to the ratio of 35:38:20:7 to obtain the final novel magnesium phosphate cement.
(5) Mixing the novel magnesium phosphate cement with water according to the water cement ratio of 0.21, adopting a cement mortar stirrer to stir at a low speed firstly and then stir at a high speed, pouring the clean slurry into a cement mortar test mold after the completion of the stirring, and curing to a specified age.
The compression strength of the magnesium phosphate cement test blocks 1d, 7d and 28d is respectively 45.86 MPa, 67.41 MPa and 77.03 MPa.
Example 3
In the embodiment, the red mud composite calcium carbonate and aluminum components are adopted to prepare the material mainly containing C4The intermediate component of AF ore phase, together with commercial dead-burned magnesia, ammonium dihydrogen phosphate and borax, is prepared into magnesium phosphate cement, which mainly comprises the following production steps:
(1) according to the weight portion, 46 portions of limestone, 38 portions of red mud and 16 portions of aluminum oxide clinker are uniformly mixed, ground and sieved by a 100-mesh sieve to obtain raw materials, and then the raw materials are ground together by a ball mill, wherein the fineness is controlled below 75 mu m.
(2) Adding water into the ground material, wetting, pressing into a test cake, standing, drying, calcining in a high-temperature furnace at 1250 ℃, keeping the temperature for 10min, putting into a ball mill after the firing, and grinding again, wherein the fineness is controlled not to exceed 75 mu m.
(3) 35 parts of the above-mentioned calcined product with C4AF is a mixture of main mineral phases, and is mixed uniformly with 40 parts of commercial dead burned magnesia, 29 parts of phosphate and 6 parts of borax to prepare magnesium phosphate cement.
(4) Mixing the phosphate with water, wherein the water cement ratio is 0.19, pouring the cement paste into a cement mortar test mold, and testing the compressive strength of the cement mortar after curing to a specified age.
The novel magnesium phosphate cement is tested for the compressive strength of 1d, 7d and 28d, and the results are respectively 38.23MPa, 54.16 MPa and 67.69 MPa.
Comparative example 1
The comparative example is a formulation of magnesium phosphate cement using commercially available raw materials, comprising the steps of:
(1) according to parts by weight, 72 parts of commercial dead burned magnesium oxide, 20 parts of monopotassium phosphate and 8 parts of borax are ground into particles with the particle size of about 100 meshes in advance, and then the components are mixed uniformly.
(2) And mixing the uniformly mixed magnesium phosphate cement with water, wherein the water cement ratio is 0.12, pouring the mixed magnesium phosphate cement clean slurry into a cement mortar test mold, demolding after 3 hours, and continuously maintaining in the air to a specified age.
The compression strength of the magnesium phosphate cements 1d, 7d and 28d is tested, and the corresponding strength values are 46.56MPa, 69.05MPa and 80.17 MPa.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (7)
1. The red mud-based magnesium phosphate cement is characterized in that: with C4AF solid solution, MgO, phosphate and retarding substances are used as main components, and the mineral phase comprises the following components in parts by weight: 30-50 parts of C4AF solid solution, 20-40 parts of MgO, 15-25 parts of phosphate and 0-10 parts of retarding component; wherein C is4The raw material precursor of the AF solid solution and the MgO comprises the following components in parts by weight: 30-50 parts of calcium-magnesium component, 30-45 parts of red mud, 10-20 parts of aluminum component and 0.5-2 parts of boron oxide.
2. The red mud-based magnesium phosphate cement according to claim 1, characterized in that: the calcium and magnesium component is dolomite or a mixture of calcium carbonate and magnesite.
3. The red mud-based magnesium phosphate cement according to claim 1, characterized in that: the red mud is high-iron aluminum-rich red mud.
4. The red mud-based magnesium phosphate cement according to claim 1, characterized in that: the aluminum component is at least one of aluminum ash and bauxite tailings.
5. The red mud-based magnesium phosphate cement according to claim 1, characterized in thatIn the following steps: said C4AF solid solution is C2F、C6AF2、C4AF、C6A2At least one of F having an average stoichiometry C4AF。
6. The red mud-based magnesium phosphate cement according to claim 1, characterized in that: the phosphate is at least one of potassium dihydrogen phosphate, ammonium dihydrogen phosphate and sodium dihydrogen phosphate.
7. A method for preparing the red mud-based magnesium phosphate cement of claim 1, which is characterized by comprising the following steps: the method comprises the following steps:
(1) preparation of the Green precursor according to C4Weighing red mud, calcium and magnesium components, aluminum components and boron oxide according to the proportion of AF solid solution and MgO and corresponding stoichiometry, and mixing and homogenizing;
(2) calcining the precursor of the raw material at 1000-1500 ℃ for 20 min-3 h, taking out and naturally cooling;
(3) grinding the material cooled in the step (2) to obtain C with fineness below 75um4AF solid solution-MgO mixture;
(4) c is to be4And compounding the AF solid solution-MgO mixture with phosphate and a retarding component to obtain the red mud-based magnesium phosphate cement.
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| CN115572147A (en) * | 2022-11-08 | 2023-01-06 | 北京科技大学 | Phosphate cementing material and preparation method thereof |
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